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Composites: Part A
journal homepage: www.elsevier.com/locate/compositesa
a r t i c l e i n f o a b s t r a c t
Article history: Currently, there is no established and cost-effective method for the bending characterization of continu-
Received 19 January 2016 ous fiber reinforced thermoplastic composites. Isothermal mechanical testing techniques are time and
Received in revised form 6 April 2016 labor-intensive and deliver information only about distinct points of the temperature-dependent
Accepted 18 June 2016
property curves. In this study, Dynamic Mechanical Analysis (DMA) as well as novel rheometer-based
Available online 24 June 2016
bending experiments were performed to assess temperature-dependent and viscoelastic behavior. On
the basis of the experimental results a new method was defined and validated for the efficient
Keywords:
characterization of temperature-dependent elastic bending behavior via DMA. Furthermore a linear
A. Thermoplastic resin
B. Thermomechanical
viscoelastic material model was derived from DMA experiments by means of time–temperature
C. Finite element analysis (FEA) superposition. As the material behavior proved to be of a highly viscoelastic nature, a method was
E. Forming developed to calibrate a material model, the parallel rheological framework, implemented in Abaqus.
Ó 2016 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.compositesa.2016.06.016
1359-835X/Ó 2016 Elsevier Ltd. All rights reserved.
S. Ropers et al. / Composites: Part A 90 (2016) 22–32 23
determined by the out-of-plane bending stiffness [2,4,5,7–9]. Sev- the University of Twente, which is based on the Kawabata Evalua-
eral studies [9,10] have demonstrated the importance of bending tion System and delivers promising results [18]. This latter method
stiffness in the simulation of a forming process. Since wrinkling is capable of investigating the bending stiffness at distinct temper-
is one of the most frequently occurring failures during draping, atures and deformation velocities. The rheometer bending setup
the problem needs to be addressed. was also employed in the framework of this study to acquire the
As pointed out, that material properties need to be understood bending stiffness at predefined temperatures as control values, as
and characterized in order to be able to conduct simulations with discussed in detail in Section 6.
reasonable outcomes. The simulation scale and the material model
determine the involved list of parameters. In a previous study [6]
3. DMA material characterization
the simulation software PAM-FORM, developed by the ESI Group,
was investigated with respect to the influence of different input
Dynamic Mechanical Analysis (DMA) is a mechanical testing
parameters, such as mechanical and thermal material properties.
technique that applies an oscillating deformation to a sample
The simulation is capable of the thermomechanical modeling of
under predefined environmental conditions and analyzes the
the thermoforming process. The Design of Experiments method
material response [19], to study the elastic and viscoelastic proper-
was employed to identify the most influential parameters whose
ties of the material. The method allows for the investigation of a
characterization is worth investing resources into. The Young’s
variety of mechanical and thermal properties and their tempera-
modulus, shear modulus, bending stiffness, specific heat, tool-ply
ture and frequency dependency. DMA instruments are becoming
frictional coefficient and the heat transfer coefficient were proven
even more versatile as state-of-the-art machines offer quasistatic
to be heavily influential on the simulation outcome.
measurement modes to obtain Young’s and other moduli [20],
Internal research at Volkswagen [11] as well as Melo and Rad-
along with creep and relaxation modes [21].
ford [12] have shown that some properties, such as the Young’s
DMA measures the elastic behavior of the material, i.e. stiffness,
modulus in fiber direction, are fiber dominated, meaning that they
and describes it with the storage modulus E0 , which is the in-phase
exhibit only a small temperature dependency in the investigated
component of the reaction to the applied sinusoidal deformation.
temperature range. It is sufficient to only characterize these prop-
The loss modulus E00 is the out-of-phase component describing
erties at distinct temperatures with conventional mechanical test-
the material’s ability to dissipate energy into heat, and the ratio
ing methods. Other properties, however, are matrix dominated and
of the loss to the storage modulus is the so-called tand, i.e. damping
therefore heavily temperature-dependent. Such properties are
[19].
transverse Young’s modulus, shear modulus and out-of-plane
Researchers use DMA to characterize polymers usually below
bending stiffness. The characterization of the shear modulus and
their melting temperature. Melo et al. [12] investigated the vis-
the bending stiffness is particularly challenging, especially due to
coelastic properties of unidirectional carbon fiber reinforced PEEK
their additional deflection and shear rate dependencies. There is
tapes, but only at a temperature range below the matrix materials
no established method for the efficient characterization of these
glass transition temperature (T g ). Other studies [22,23] employed
properties [8].
DMA to examine the temperature-dependent elastic moduli of
epoxies and to compare them to conventional mechanical testing
data. They found discrepancies between the actual values but good
2. Methods for bending characterization
correlation between their temperature dependencies. Margossian
et al. [5] presented a DMA-based characterization method for the
The bending stiffness of continuous materials is classically
bending behavior of unidirectional composite tapes. The study
derived from their in-plane properties [13]. However, the investi-
was conducted under the assumption that experimental forming
gations of Yu et al. [14] have shown that the calculated bending
methods are mostly modeled as isothermal processes. Thus, the
stiffness is unrealistically high compared to the experimentally
study focuses on characterizing the material’s bending behavior
obtained value of a fiber-reinforcement. This can be attributed to
at distinct temperatures, instead of doing temperature sweeps over
sliding mechanisms between the yarns and individual fibers of
a broader range. Such a characterization method yields insufficient
the reinforcement, which assign a specific bending behavior to
data for thermomechanical simulations. A great number of isother-
the reinforcement that is independent of the tensile and shear
mal measurements would be required to characterize the temper-
properties and, therefore, cannot be deduced from the calculated
ature range in question, which brings us back to the inefficiency of
values [9,15]. Modern simulation software and material models
common mechanical testing techniques.
are aware of that and require an independent bending stiffness
The method proposed in this study enables the fast and efficient
to be defined for main fiber directions. Thus, bending characteriza-
characterization of both temperature and frequency dependencies
tion is a vital requirement for forming simulations.
of the bending stiffness, however, it does not deliver the actual
Only few studies have been carried out to date on the bending
bending stiffness values. The technique requires the bending stiff-
characterization of continuous fiber reinforced thermoplastic com-
ness to be determined at least at one temperature within the inves-
posites in their molten state [5,9,10,16]. Conventional bending test
tigated range.
methods are inapplicable to materials with low bending stiffness
such as dry reinforcement fabrics and molten state thermoplastic
prepregs. The testing techniques developed by the textile industry 4. Materials and instruments
were used as the basis for the development of techniques applica-
ble to such materials. Most bending characterization techniques All experiments were performed on two materials; both
are based on the cantilever or the Kawabata tests, which both orig- representing the most commonly used thermoplastic prepreg
inate from the textile industry. Several studies employed a modi- types. The first investigated material is a woven textile reinforced
fied version of the cantilever test to characterize the bending thermoplastic prepreg (TPP) material, Tepex 102 dynalite-RG600
behavior, such as those conducted by Boisse [4] or Peirce [17]. Mar- (x)/47% supplied by Bond-Laminates. The prepreg consist of a 2/2
gossian [5] presented an extensive review of the existing test twill glass fiber weave impregnated with a polyamide 6 (PA6)
methods for bending characterization, explaining various versions matrix. Main properties of the material are listed in the material
of the cantilever test, the Kawabata test and the V-bending test. data sheet provided by the manufacturer [24] and listed in Table 1.
The study also mentions the modified rheometer developed by The second material is a continuous unidirectional carbon fiber
24 S. Ropers et al. / Composites: Part A 90 (2016) 22–32
5. Implementation
Fig. 1. Experimental set-up in rheometer for bending experiments [18]. Fig. 2. Dynamic mechanical analysis: dual cantilever fixture.
S. Ropers et al. / Composites: Part A 90 (2016) 22–32 25
was used. The heating rate was set to 1.5 K min1 during the exper- Table 2
iments. The environmental chamber was continuously flushed Investigated materials and parameters in rheometer bending tests.
with nitrogen in order to avoid polymer oxidation at elevated Materials Temperatures (°C) Rotational velocities (rpm)
temperatures. Tepex 60/150/210/220/ 0.1/1/10
Temperature-sweeps were conducted from 150 °C to 260 °C. Ultratape 210+/220+/260
150 °C was chosen as the lower limit of the investigated tempera-
ture range, as it is a favorable mold temperature for thermoform-
ing PA6 materials. It is very unlikely that the blank temperature tional velocities will further be referred to as 0.1 rpm (rotations
would drop below 150 °C during the swift forming process. The per minute), 1 rpm and 10 rpm.
upper limit was chosen to be 260 °C, because this is the upper limit Crystal melting is an endothermic transition, while crystalliza-
of the processing temperature range defined by the prepreg man- tion is exothermic. When cooling the environmental chamber from
ufacturer. At higher temperatures the matrix material is prone to above the melting temperature, the sample will consolidate and
temperature degradation; furthermore, the mechanical properties crystallize, while giving off heat. This keeps the sample warm
are not changing significantly once complete melting has occurred. and shifts the apparent melting temperature to a lower value.
Six frequencies from 0.1 Hz to 10 Hz were investigated: 0.1, 0.5, Therefore, bending tests around melting temperature T m were per-
1, 2, 5 and 10 Hz. The maximum amplitude of the employed DMA formed both while heating up and while cooling down after over-
instrument is 0.24 mm. It takes a quarter of the cycle time for the heating. As expected, the experiments conducted while cooling the
stamp to get from the initial position to the maximum amplitude. sample from a temperature > T m delivered significantly lower
At a 10 Hz frequency this means that the sample is flexed 0.24 mm mechanical properties, as the material still exhibited molten state
in 0.025 s, which roughly corresponds to a punch velocity of behavior. Thus, tests were performed at 60 °C, 150 °C, 210 °C,
10 mm s1. The actual strain rate of the blank during draping is 220 °C and 260 °C without overheating, furthermore, at 210 °C
geometry dependent and non-uniform, but this has not been and 220 °C with overheating to 255 °C and cooling back to 210 °C
accounted for in this study. This is a necessary simplification in and 220 °C (indicated with ‘‘+” henceforth and in Table 2), respec-
order to limit the complexity of the model. tively, to identify the shift in behavior due to crystallization and
Five experiments were made for both directions and both mate- crystal melting. After reaching the experimental temperature, a
rial types. According to the material data sheet, there is a small dif- two minute balancing time was employed to ensure a homoge-
ference between mechanical properties in weft and warp neous temperature field in the sample during the test. The mea-
directions. This can be attributed to the prepreg manufacturing sured temperature, however, might differ from the actual sample
technique that pulls the weft rovings out of alignment by slightly temperature during the measurements, due to the following
bending them. This difference was investigated by conducting reasons:
DMA measurements on samples cut in both directions. The result-
ing difference was deemed to be negligible, henceforth only warp Temperature sensor was not inside/not in contact with the
direction results were taken into account. sample.
The result of DMA measurements are the complex modulus E Heating rate was relatively high.
with its real and imaginary parts E0 and E00 which denote the stor- Balancing time might not be sufficient to reach homogeneous
age and loss modulus respectively. temperature field.
E ¼ E0 þ ıE00 ð1Þ
6. Experimental results
0
The storage modulus E describes the material’s ability to store
the deformation energy while the loss modulus E00 describes the In the following section the results of DMA bending and
ratio of the deformation energy which is transformed into heat rheometer experiments will be presented.
by dissipation. Their ratio is usually referred to as tan d or damping.
6.1. DMA experiments
E00
tan d ¼ ð2Þ
E0 Twenty DMA measurements were made; five for both direc-
tions for both materials. As previously discussed, only warp direc-
tion results of the fabric and longitudinal results of the tape are
5.2. Rheometer bending experiments
considered in the analysis. The storage modulus values of the five
identical measurements were averaged for every frequency tested.
The rheometer bending setup was used in the scope of this
Three frequencies are being further investigated: 0.1, 1 and 10 Hz.
work to investigate the bending behavior of single plies of Tepex
These roughly correspond to the angular velocities used in the
and Ultratape material. Additionally to the experimental procedure
rheometer measurements. Fig. 4 shows the average storage and
performed by Sachs, relaxation was also investigated. After bend-
loss modulus as well as damping curves for these three frequen-
ing the specimen from 0° to 70° the bending angle was held at
cies. The damping exhibits more distinctive frequency dependence
70° for another 120 s, while measuring the reaction moment.
owing to the viscous behavior of the molten thermoplastic.
Fig. 3 gives an overview of the test procedure:
These averaged storage modulus values were then converted
The tested parameters and their settings are listed in Table 2.
Three bending rates were tested at five temperatures. The rota- into proportionality P i factors by dividing every value E0i with the
base value E0base , i.e. the storage modulus corresponding to the low-
est investigated temperature:
E0 ðT i Þ
PðT i Þ ¼ : ð3Þ
E0 ðT base Þ
Thus, an array of proportionality factors starts with a value of
one (corresponding to the base temperature) and gradually
Fig. 3. Rheometer bending test procedure. decreases to a value less than one, which shows how much smaller
26 S. Ropers et al. / Composites: Part A 90 (2016) 22–32
Fig. 8. Fluctuations in moment signals due to inertia of instrument and sample holder.
Fig. 13. Simulated and experimental maximum bending moments at speed 10 rpm versus temperature.
moment and bending angle results were extracted for every incre-
ment. Thus, the correlation between logarithmic strain and bend-
ing angle as well as stress and reaction moment was established,
separately for each bending velocity. On the basis of this correla-
tion, strains and the ratios of stresses to reaction moments were
linearly interpolated corresponding to the bending angles of the
rheometer measurements. The resulting ratios of stress to reaction
moment were multiplied with the reaction moments from the
rheometer measurements, thus delivering the stress values corre-
sponding to the strains. The resulting stress–strain data was used
to calibrate the material model employed in the simulations to cor-
respond to the experimental results. The calibration was done via
an automated iteration process. The obtained material model has
then been implemented in the subsequent array of simulations.
This process was repeated until the simulation results showed an
acceptable correlation to the experiments. Such a process is shown
in Fig. 15. The same material model parameters were used for all
Fig. 16. Experimental and simulated bending moment of Tepex at 220 °C and 1 rpm
rotational velocities. The corresponding result for the 1 rpm speed rotational velocity.
is depicted in Fig. 16.
Figs. 15 and 16 clarify, that a non-linear viscoelastic material
model is capable of representing the actual material bending
behavior of thermoplastic prepregs. The results delivered by the
employed parallel rheological framework not only fit the experi-
mental results during the deformation of the specimen but also
accurately represent the relaxation behavior. The developed
method of coupling an iterative process with a calibration algo-
rithm allows for an efficient and robust determination of material
model parameters.
Fig. 18. Experimental and simulated bending moment of Tepex at 210 °C and 1 rpm
rotational velocity.
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